We study possible modification of synthesized iron oxide (Fe 3 O 4 ) nanoparticles (NPs) with organic molecules of citric acid (CA) and vitamin C (ascorbic acid), and then incorporation of dicapped magnetic NPs into valuable poly(vinyl alcohol) (PVA) matrix. Biocompatible CA and ascorbic acid (AS) coupling agents can create organic functional groups on the surface of Fe 3 O 4 NPs for better interfacial compatibility with the organic polymer matrix. Magnetic PVA@Fe 3 O 4 /CA/AS nanocomposite (NC) films containing 4, 8, and 12 wt% of the modified NPs were successfully manufactured by a fast, green, and safe strategy under ultrasonic irradiation. Surface functionality groups, morphology of the modified NPs, and also the fabricated NCs were analyzed by Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis, X-ray diffraction, UV-Visible spectroscopy, field emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM). In comparison to the pure PVA, the PVA@Fe 3 O 4 /CA/AS NCs were shown to have higher decomposition temperature. With incorporation of 4 wt % Fe 3 O 4 , the tensile strength and Young's modulus of the NC have significantly improved compared with PVA. In addition, the surface morphology images showed that NPs were dispersed homogenously into the polymer matrix at nanoscale.